JP6063376B2 - Sliding member - Google Patents

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JP6063376B2
JP6063376B2 JP2013502237A JP2013502237A JP6063376B2 JP 6063376 B2 JP6063376 B2 JP 6063376B2 JP 2013502237 A JP2013502237 A JP 2013502237A JP 2013502237 A JP2013502237 A JP 2013502237A JP 6063376 B2 JP6063376 B2 JP 6063376B2
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dlc film
friction
members
sliding
steel
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JPWO2012117854A1 (en
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健太郎 小森
健太郎 小森
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Honda Motor Co Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H57/00—General details of gearing
    • F16H57/04—Features relating to lubrication or cooling or heating
    • F16H57/0463—Grease lubrication; Drop-feed lubrication
    • F16H57/0464—Grease lubrication
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/02—Parts of sliding-contact bearings
    • F16C33/04—Brasses; Bushes; Linings
    • F16C33/06—Sliding surface mainly made of metal
    • F16C33/10—Construction relative to lubrication
    • F16C33/102—Construction relative to lubrication with grease as lubricant
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/02—Parts of sliding-contact bearings
    • F16C33/04—Brasses; Bushes; Linings
    • F16C33/06—Sliding surface mainly made of metal
    • F16C33/12—Structural composition; Use of special materials or surface treatments, e.g. for rust-proofing
    • F16C33/122—Multilayer structures of sleeves, washers or liners
    • F16C33/124—Details of overlays
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H57/00—General details of gearing
    • F16H57/04—Features relating to lubrication or cooling or heating
    • F16H57/041—Coatings or solid lubricants, e.g. antiseize layers or pastes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
    • C10M2219/068—Thiocarbamate metal salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/045—Metal containing thio derivatives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/042—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for automatic transmissions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
    • C10N2040/044—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives for manual transmissions
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/25—Internal-combustion engines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Semi-solids; greasy
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16H—GEARING
    • F16H19/00—Gearings comprising essentially only toothed gears or friction members and not capable of conveying indefinitely-continuing rotary motion
    • F16H19/02—Gearings comprising essentially only toothed gears or friction members and not capable of conveying indefinitely-continuing rotary motion for interconverting rotary or oscillating motion and reciprocating motion
    • F16H19/04—Gearings comprising essentially only toothed gears or friction members and not capable of conveying indefinitely-continuing rotary motion for interconverting rotary or oscillating motion and reciprocating motion comprising a rack

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Lubricants (AREA)
  • Sliding-Contact Bearings (AREA)
  • Chemical Vapour Deposition (AREA)

Description

本発明は、原動機や動力伝達装置などに用いられる摺動部材に係り、相対する二つの部材の間に潤滑添加剤を含有するグリースを介在させて互いに摺動する摺動部材に関する。   The present invention relates to a sliding member used in a prime mover, a power transmission device, and the like, and more particularly to a sliding member that slides on each other with a grease containing a lubricant additive interposed between two opposing members.

原動機や動力伝達装置などに用いられる摺動部材については、互いに摺動する部材の保護や燃費向上を通じた地球環境保護を目的として、摩擦を減らすための研究が精力的に進められており、数多くの手法が提案されている。例えば、浸炭処理、窒化処理、セラミックス硬質皮膜処理などは前記した目的のためによく用いられる手法である。   With regard to sliding members used in prime movers and power transmission devices, many studies are underway to reduce friction with the aim of protecting the global environment through protecting each other's sliding members and improving fuel efficiency. This method has been proposed. For example, carburizing treatment, nitriding treatment, ceramic hard coating treatment, and the like are techniques often used for the above-described purposes.

近年では、摺動部材の表面にＤＬＣ膜を形成すると、摺動時にＤＬＣ膜の炭素成分がグラファイト化して固体潤滑剤として機能し、低摩擦化できることに注目が集まり、研究報告等が盛んに行われている。   In recent years, when a DLC film is formed on the surface of a sliding member, attention has been paid to the fact that the carbon component of the DLC film is graphitized during sliding to function as a solid lubricant, reducing friction, and research reports have been actively conducted. It has been broken.

例えば、特許文献１や特許文献２には、互いに摺動する摺動部材の一部に非晶質硬質炭素膜（ダイヤモンドライクカーボン膜（ＤＬＣ膜）とも呼ばれる。）を形成することが記載されている。   For example, Patent Document 1 and Patent Document 2 describe forming an amorphous hard carbon film (also called a diamond-like carbon film (DLC film)) on a part of sliding members that slide with each other. Yes.

また、例えば、特許文献３には、互いに摺動する摺動部材の表面に、アークイオンプレーティング（ＡＩＰ）法により第１のＤＬＣ膜と第２のＤＬＣ膜を順に被覆することが記載されている。また、第１のＤＬＣ膜の表面硬さをナノインデンテーション試験で２０〜３０ＧＰａとし、第２のＤＬＣ膜の表面硬さを７０〜９０ＧＰａとすることが記載されている。   For example, Patent Document 3 describes that the surfaces of sliding members that slide relative to each other are sequentially coated with a first DLC film and a second DLC film by an arc ion plating (AIP) method. Yes. Further, it is described that the surface hardness of the first DLC film is set to 20 to 30 GPa in the nanoindentation test, and the surface hardness of the second DLC film is set to 70 to 90 GPa.

さらに、例えば、特許文献４には、非有機モリブデン系固体潤滑剤と非セッケン系増ちょう剤を含むグリースを介在させて互いに摺動する摺動部材のうちの一方の部材の表面にＤＬＣ膜を形成することが記載されている。   Further, for example, in Patent Document 4, a DLC film is formed on the surface of one of sliding members that slide on each other with a grease containing a non-organic molybdenum-based solid lubricant and a non-soap-based thickener interposed therebetween. It is described to form.

特開２００７−１５４１２号公報JP 2007-15154 A 特開２００９−１０３１９０号公報JP 2009-103190 A 特開２００８−３２１５０号公報JP 2008-32150 A 国際公開第２０１０／０５２７８７号パンフレットInternational Publication No. 2010/052787 Pamphlet

しかしながら、特許文献１、２には、ＤＬＣ膜の条件や製造手法、効果などが記載されていないため、十分に低摩擦化できないおそれがあった。   However, Patent Documents 1 and 2 do not describe the DLC film conditions, manufacturing method, effects, and the like.

また、特許文献３には、ＡＩＰ法を用いたＤＬＣ膜の形成が記載されているが、物理蒸着による方法であり、優れた膜物性を有する反面、蒸着源の指向性が大きく、被覆する部材の形状や同時に処理可能な数量が限定される。さらに、潜在的に非常に高硬度で、かつ表面が過度に粗くなる性質があり、相手攻撃性の抑制が難しく、成膜後の研磨工程等が必要になることが多く、コストも必要になる。そのために安価で簡便にこれを形成することが困難であった。   Patent Document 3 describes the formation of a DLC film using the AIP method, which is a method by physical vapor deposition, which has excellent film properties, but has a high directivity of the vapor deposition source and is a covering member. The shape and quantity that can be processed simultaneously are limited. Furthermore, it is potentially very hard and has a property that the surface becomes excessively rough, it is difficult to suppress the partner's aggression, a polishing step after film formation is often required, and costs are also required. . Therefore, it was difficult to form this easily and inexpensively.

そして、特許文献４に記載の技術は、低摩擦化の効果を奏するために潤滑添加剤を添加したグリースを用いているが、当該潤滑添加剤として添加できる成分が特定のものに制限されるだけでなく、十分に低摩擦化できないおそれがあった。   The technique described in Patent Document 4 uses a grease to which a lubricating additive is added in order to achieve the effect of reducing friction, but the components that can be added as the lubricating additive are limited to specific ones. In addition, there was a risk that the friction could not be reduced sufficiently.

本発明は前記状況に鑑みてなされたものであり、安価且つ簡便でありながら低摩擦性に優れた摺動部材を提供することを課題とする。   This invention is made | formed in view of the said condition, and makes it a subject to provide the sliding member excellent in the low friction property, being cheap and simple.

前記課題を解決した本発明は、相対する二つの部材の間にジアルキルジチオカルバミン酸モリブデン、ジチオリン酸モリブデン、二硫化モリブデン、ポリテトラフルオロエチレンのうちの少なくとも一つを潤滑添加剤として含有し、銅系の添加剤を含有しないグリースを介在させて互いに摺動する摺動部材であって、前記二つの部材のうちの少なくとも一つの部材の摺動面に、水素を１７〜２９原子％含み、ヤング率が２０１ＧＰａ以上２５３ＧＰａ以下、膜厚が０．５〜２０μｍである非晶質硬質炭素膜を形成したことを特徴としている。
また、本発明は、相対する二つの部材の間にジアルキルジチオカルバミン酸モリブデン、ジチオリン酸モリブデン、二硫化モリブデン、ポリテトラフルオロエチレンのうちの少なくとも一つを潤滑添加剤として含有し、銅系の添加剤を含有しないグリースを介在させて互いに摺動する摺動部材であって、前記二つの部材のうちの少なくとも一つの部材の摺動面に、水素を含み、ヤング率が２０１ＧＰａ以上２５３ＧＰａ以下、前記グリースを介在させた摩擦係数が０．０５７以上０．１０６以下、膜厚が０．５〜２０μｍである非晶質硬質炭素膜を形成したことを特徴としている。 The present invention has solved the above problems, molybdenum dialkyldithiocarbamate between two opposite members, molybdenum dithiophosphate, contains molybdenum disulfide, at least one of polytetrafluoroethylene as a lubricant additive, copper-based A sliding member that slides on each other with a grease that does not contain any additive , wherein the sliding surface of at least one of the two members contains 17 to 29 atomic% of hydrogen, and has a Young's modulus Is characterized in that an amorphous hard carbon film having a thickness of 201 to 253 GPa and a film thickness of 0.5 to 20 μm is formed.
The present invention also includes at least one of molybdenum dialkyldithiocarbamate, molybdenum dithiophosphate, molybdenum disulfide, and polytetrafluoroethylene as a lubricating additive between two opposing members, and a copper-based additive A sliding member that slides on each other with a grease that does not contain hydrogen, wherein the sliding surface of at least one of the two members contains hydrogen and has a Young's modulus of 201 GPa to 253 GPa, An amorphous hard carbon film having a friction coefficient of 0.057 to 0.106 and a film thickness of 0.5 to 20 μm is formed.

前記した数値範囲のヤング率を有する非晶質硬質炭素膜は、比較的硬質でありながら適度な硬さを有している。そのため、摺動部材が摺動して摩擦が起きると、非晶質硬質炭素膜の炭素成分の黒鉛質物質への構造変化やグリースに含有されている潤滑添加剤の摩擦化学反応を促進することができる。なお、摩擦化学反応とは、摩擦によって生じる圧力や摩擦熱によって進められる化学反応のことをいう。
構造変化して得られた黒鉛質物質や潤滑添加剤が摩擦化学反応により形成した物質は、いずれも層状構造物質であり、摩擦界面や摩擦によって生成されたトライボフィルムは、これらが混在した状態になる。
本発明では、比較的硬質でありながら適度な硬さを有する非晶質硬質炭素膜を、構造変換や摩擦化学反応に、積極的に関与させることによって、摩擦界面や部材表面に異なる複数の層状構造物質相を十分に生成させ、混在させる。混在する各層状構造物質は、それぞれ異なる摩擦特性を有していると考えられるため、これらが十分に生成され、混在することによって、その効果を重畳的に得ることができる結果、より幅広い範囲で安定して低摩擦化を図ることが可能となる。また、水素を含む非晶質硬質炭素膜でよいので、ＡＩＰ法によるよりも安価且つ簡便にこれを得ることができる。The amorphous hard carbon film having the Young's modulus in the numerical range described above has an appropriate hardness while being relatively hard. Therefore, when friction occurs due to sliding of the sliding member, the structural change of the carbon component of the amorphous hard carbon film to the graphite material and the tribochemical reaction of the lubricating additive contained in the grease are promoted. Can do. The frictional chemical reaction refers to a chemical reaction that is advanced by pressure generated by friction or frictional heat.
Graphite materials obtained by structural changes and materials formed by tribochemical reaction of lubricating additives are all layered structural materials, and tribofilms produced by friction interfaces and friction are in a state where they are mixed. Become.
In the present invention, an amorphous hard carbon film that is relatively hard but has an appropriate hardness is actively involved in structural transformations and tribochemical reactions, whereby a plurality of different layers are formed on the friction interface and the member surface. Fully generate and mix the structural material phase. Each layered structure material that is mixed is considered to have different frictional characteristics, so that they can be generated sufficiently and mixed to obtain their effects in a broader range. It is possible to stably reduce friction. Further, since an amorphous hard carbon film containing hydrogen may be used, it can be obtained more easily and cheaply than by the AIP method.

本発明によれば、安価且つ簡便でありながら低摩擦性に優れた摺動部材を提供することができる。   According to the present invention, it is possible to provide a sliding member that is inexpensive and simple and has excellent low friction properties.

本発明の一実施形態に係る摺動部材の一例を示す断面図である。It is sectional drawing which shows an example of the sliding member which concerns on one Embodiment of this invention. ボールオンディスク摩擦摩耗試験の様子を説明する説明図である。It is explanatory drawing explaining the mode of a ball-on-disk friction abrasion test. 実施例１〜４および比較例１〜６のヤング率と摩擦係数に関するグラフである。なお、横軸はヤング率［ＧＰａ］であり、縦軸は摩擦係数である。◆および◇のプロットは、潤滑添加剤としてＰＴＦＥを添加していることを表し、■のプロットは、潤滑添加剤としてＭｏ系を添加していることを表し、○のプロットは、潤滑添加剤を添加していないことを表す。It is a graph regarding the Young's modulus and friction coefficient of Examples 1-4 and Comparative Examples 1-6. The horizontal axis represents Young's modulus [GPa], and the vertical axis represents the friction coefficient. The ◆ and ◇ plots indicate that PTFE is added as a lubricant additive, the ■ plots indicate that a Mo-based additive is added as a lubricant additive, and the ○ plots indicate that a lubricant additive is added. This means that it has not been added. 実施例１〜４および比較例１〜６のＤＬＣ膜の水素含有量と摩擦係数に関するグラフである。なお、横軸は水素含有量［ａｔ％］であり、縦軸は摩擦係数である。◆および◇のプロットは、潤滑添加剤としてＰＴＦＥを添加していることを表し、■および□のプロットは、潤滑添加剤としてＭｏ系を添加していることを表し、○のプロットは、潤滑添加剤を添加していないことを表す。It is a graph regarding the hydrogen content of the DLC film of Examples 1-4 and Comparative Examples 1-6, and a friction coefficient. The horizontal axis represents the hydrogen content [at%], and the vertical axis represents the friction coefficient. ◆ and ◇ plots indicate that PTFE is added as a lubricant additive, ■ and □ plots indicate that a Mo-based additive is added as a lubricant additive, and ○ plots indicate that a lubricant is added Indicates that no agent is added. 実施例５と比較例７のフリクショントルクを測定した結果を示すグラフである。なお、横軸はピニオンギア部品の角度［°］を表し、縦軸はフリクショントルク［Ｎ・ｍ］を表す。It is a graph which shows the result of having measured the friction torque of Example 5 and Comparative Example 7. FIG. The horizontal axis represents the angle [°] of the pinion gear part, and the vertical axis represents the friction torque [N · m].

本発明の主旨は、摺動面における非晶質硬質炭素膜とグリース中の潤滑添加剤の組み合わせにおいて、非晶質硬質炭素膜のヤング率を向上させて潤滑添加剤との摩擦反応を積極的に起こすことで良好な摩擦層を形成し、低摩擦化を図ることにある。   The gist of the present invention is that the combination of the amorphous hard carbon film on the sliding surface and the lubricating additive in the grease improves the Young's modulus of the amorphous hard carbon film and actively causes a friction reaction with the lubricating additive. This is to form a good friction layer by reducing the friction and to reduce the friction.

次に、適宜図面を参照して、本発明の一実施形態に係る摺動部材について詳細に説明する。
図１は、摺動部材の一例として、ステアリング装置のラックアンドピニオン摺動機構を、ラックの軸方向と平行且つラックに設けられた歯車に対して垂直な方向に切断した断面図である。Next, a sliding member according to an embodiment of the present invention will be described in detail with reference to the drawings as appropriate.
FIG. 1 is a cross-sectional view of a rack and pinion sliding mechanism of a steering device as an example of a sliding member, cut in a direction parallel to the axial direction of the rack and perpendicular to a gear provided on the rack.

図１に図示する摺動部材１は、相対する二つの部材２、３の間にグリース４を介在させて互いに摺動するものであって、前記した二つの部材２、３のうちの少なくとも一つの部材（図１においては、部材２）の摺動面２ａに、非晶質硬質炭素膜（以下単に、「ＤＬＣ膜」という。）５を形成している。   A sliding member 1 shown in FIG. 1 slides with a grease 4 interposed between two opposing members 2 and 3, and is at least one of the two members 2 and 3 described above. An amorphous hard carbon film (hereinafter simply referred to as “DLC film”) 5 is formed on the sliding surface 2a of one member (member 2 in FIG. 1).

ＤＬＣ膜５のヤング率は、２００ＧＰａ以上３００ＧＰａ以下であることが必要である。ＤＬＣ膜５のヤング率がこの範囲にあれば、比較的硬質でありながら適度な硬さを有しているため、摺動部材１が摺動して摩擦が起きると、ＤＬＣ膜５の炭素成分の黒鉛質物質への構造変化や潤滑添加剤の摩擦化学反応を促進することができる。   The Young's modulus of the DLC film 5 needs to be 200 GPa or more and 300 GPa or less. If the Young's modulus of the DLC film 5 is within this range, it is relatively hard but has an appropriate hardness. Therefore, when the sliding member 1 slides and causes friction, the carbon component of the DLC film 5 It is possible to promote the structural change of the graphite to a graphite substance and the tribochemical reaction of the lubricant additive.

ＤＬＣ膜５のヤング率が２００ＧＰａ未満であると、ＤＬＣ膜５が軟らか過ぎるため、ＤＬＣ膜５の炭素成分の黒鉛質物質への構造変化が不十分であり、同時に、潤滑添加剤の摩擦化学反応が十分に進行しないため、低摩擦化を図ることができない。
一方、ＤＬＣ膜５のヤング率が３００ＧＰａを超えると、ＤＬＣ膜５の炭素成分の黒鉛質物質への構造変化や潤滑添加剤の摩擦化学反応を促進するには十分であるものの、相手攻撃性が大きくなり過ぎるため、長期使用により相手材の摩耗が激しくなることが予想されるので好ましくない。
ＤＬＣ膜５のヤング率は、２２５ＧＰａとするのが好ましく、２４７ＧＰａとするのがより好ましく、２５３ＧＰａとするのがさらに好ましい。
ヤング率は、ＩＳＯ １４５７７に準拠したナノインデンテーション法で測定することができ、精度よく算出することができる。When the Young's modulus of the DLC film 5 is less than 200 GPa, since the DLC film 5 is too soft, the structural change of the carbon component of the DLC film 5 to the graphite material is insufficient, and at the same time, the tribochemical reaction of the lubricant additive However, the friction cannot be reduced.
On the other hand, if the Young's modulus of the DLC film 5 exceeds 300 GPa, the DLC film 5 is sufficient to promote the structural change of the carbon component of the DLC film 5 to the graphite material and the tribochemical reaction of the lubricant additive, Since it becomes too large, it is expected that the wear of the mating material will become severe due to long-term use.
The Young's modulus of the DLC film 5 is preferably 225 GPa, more preferably 247 GPa, and even more preferably 253 GPa.
The Young's modulus can be measured by a nanoindentation method based on ISO 14577, and can be calculated with high accuracy.

ＤＬＣ膜５の硬さを示すヤング率は、ＤＬＣ膜５中の水素含有量とよい相関性がある。つまり、ＤＬＣ膜５中の水素含有量が多いとＤＬＣ膜５のヤング率は低くなる傾向があり、ＤＬＣ膜５中の水素含有量が少ないとＤＬＣ膜５のヤング率が高くなる傾向がある。ＤＬＣ膜５のヤング率が前記したように２００ＧＰａ以上３００ＧＰａ以下の範囲である場合、原料ガス、ガス圧力、成膜時間、バイアス電圧、プラズマ出力などの成膜条件によっても若干異なるが、ＤＬＣ膜５中の水素含有量は１７〜２９ａｔ％（原子％）程度とすればよい。
なお、ＤＬＣ膜５の膜厚は０．５〜２０μｍ程度あれば、前記した作用効果を奏することができる。ＤＬＣ膜５の好ましい膜厚は１〜１０μｍ程度である。The Young's modulus indicating the hardness of the DLC film 5 has a good correlation with the hydrogen content in the DLC film 5. That is, if the hydrogen content in the DLC film 5 is large, the Young's modulus of the DLC film 5 tends to be low, and if the hydrogen content in the DLC film 5 is small, the Young's modulus of the DLC film 5 tends to be high. When the Young's modulus of the DLC film 5 is in the range of 200 GPa or more and 300 GPa or less as described above, the DLC film 5 is slightly different depending on the film forming conditions such as source gas, gas pressure, film forming time, bias voltage, and plasma output. The hydrogen content therein may be about 17 to 29 at% (atomic%).
In addition, if the film thickness of the DLC film 5 is about 0.5-20 micrometers, there can exist the above-mentioned effect. A preferable film thickness of the DLC film 5 is about 1 to 10 μm.

かかるＤＬＣ膜５は、例えば、プラズマＣＶＤ（Chemical Vapor Deposition）法によって形成することができる。ＤＬＣ膜５を形成するための原料ガスとしては、メタン（ＣＨ4）、アセチレン（Ｃ2Ｈ2）、ベンゼン（Ｃ6Ｈ6）やトルエン（Ｃ7Ｈ8）などを用いることができる。ガス圧力は０．４〜２．２Ｐａなどとすることができる。成膜時間は３０〜２６０ｍｉｎ、バイアス電圧は５００〜２０００Ｖ、プラズマ出力は２０〜２００Ｗなどとすることができる。The DLC film 5 can be formed by, for example, a plasma CVD (Chemical Vapor Deposition) method. As a source gas for forming the DLC film 5, methane (CH 4 ), acetylene (C 2 H 2 ), benzene (C 6 H 6 ), toluene (C 7 H 8 ), or the like can be used. The gas pressure can be 0.4 to 2.2 Pa or the like. The film formation time may be 30 to 260 min, the bias voltage may be 500 to 2000 V, the plasma output may be 20 to 200 W, and the like.

相対する二つの部材２、３は、いわゆる普通鋼や特殊鋼などの鉄鋼材料で形成されたものであればどのようなものも用いることができる。また、非鉄金属やセラミックなどで形成することもできる。   As the two opposing members 2 and 3, any member can be used as long as it is formed of a steel material such as so-called ordinary steel or special steel. It can also be formed of non-ferrous metal or ceramic.

普通鋼としては、日本工業規格（ＪＩＳ）で規格されている一般構造用圧延鋼材（ＳＳ材）、溶接構造用圧延鋼材（ＳＭ材）、ボイラーおよび圧力容器用鋼材（ＳＢ材）、高圧ガス容器用鋼板および鋼帯（ＳＧ材）、熱間圧延鋼材および鋼帯（ＳＰＨ材）、鋼管用熱間圧延炭素鋼鋼帯（ＳＰＨＴ材）、自動車構造用熱間圧延鋼板および鋼帯（ＳＡＰＨ材）、冷間圧延鋼板および鋼帯（ＳＰＣ材）などを挙げることができる。   Common steel includes rolled steel for general structure (SS material), rolled steel for welded structure (SM material), boiler and pressure vessel steel (SB material), and high-pressure gas container. Steel plate and steel strip (SG material), hot rolled steel material and steel strip (SPH material), hot rolled carbon steel strip for steel pipes (SPHT material), automotive structural hot rolled steel plate and steel strip (SAPH material) And cold rolled steel sheets and steel strips (SPC materials).

また、特殊鋼としては、高炭素クロム軸受鋼（ＳＵＪ２材）、クロムモリブデン鋼鋼材（ＳＣＭ材）が好ましいが、機械構造用炭素鋼（Ｓ−Ｃ材）、炭素工具鋼鋼材（ＳＫ材）、切削工具用合金工具鋼鋼材（ＳＫＳ材）、冷間ダイス用合金工具鋼鋼材（ＳＫＤ材）、熱間金型用合金工具鋼鋼材（ＳＫＴ材）、高速度工具鋼鋼材（ＳＫＨ材）、炭素クロム軸受鋼鋼材（ＳＵＪ材）、ばね鋼鋼材（ＳＵＰ材）、ステンレス鋼鋼材（ＳＵＳ材）、耐熱鋼鋼材（ＳＵＨ材）、定温圧力容器用炭素鋼鋼材（ＳＬＡ材）、磁心鋼や磁石鋼、鍛鋼品（ＳＦ材）、鋳鋼品（ＳＣ材）、鋳鉄品（ＦＣ材）などを挙げることができる。   As the special steel, high carbon chromium bearing steel (SUJ2 material) and chromium molybdenum steel steel (SCM material) are preferable, but carbon steel for machine structure (SC material), carbon tool steel (SK material), Alloy tool steel for cutting tools (SKS material), Alloy tool steel for cold dies (SKD material), Alloy tool steel for hot die (SKT material), High speed tool steel (SKH material), Carbon Chrome bearing steel (SUJ), spring steel (SUP), stainless steel (SUS), heat-resistant steel (SUH), carbon steel for constant temperature pressure vessels (SLA), magnetic core steel and magnet steel Forged steel products (SF materials), cast steel products (SC materials), cast iron products (FC materials), and the like.

非鉄金属としては、アルミニウム、マグネシウム、チタンまたはこれらから選択されるいずれか一つを主成分とする合金を挙げることができる。   Examples of the non-ferrous metal include aluminum, magnesium, titanium, and an alloy mainly containing any one selected from these.

アルミニウムまたはアルミニウム合金としては、ＪＩＳで規格されている純Ａｌ（１０００系）、Ａｌ−Ｃｕ，Ａｌ−Ｃｕ−Ｍｇ系合金（２０００系）、Ａｌ−Ｍｎ，Ａｌ−Ｍｎ−Ｍｇ系合金（３０００系）、Ａｌ−Ｓｉ−Ｃｕ−Ｍｇ−Ｎｉ，Ａｌ−Ｓｉ系合金（４０００系）、Ａｌ−Ｍｇ系合金（５０００系）、Ａｌ−Ｍｇ−Ｓｉ系合金（６０００系）、Ａｌ−Ｚｎ−Ｍｇ−Ｃｕ，Ａｌ−Ｚｎ−Ｍｇ系合金（７０００系）、Ａｌ−Ｃｕ合金（ＡＣ１Ａ）、Ａｌ−Ｃｕ−Ｍｇ合金（ＡＣ１Ｂ）、Ａｌ−Ｃｕ−Ｍｇ−Ｎｉ合金（ＡＣ５Ａ）、Ａｌ−Ｓｉ合金（ＡＣ３Ａ、ＡＤＣ１）、Ａｌ−Ｃｕ−Ｓｉ合金（ＡＣ２Ａ、ＡＣ２Ｂ）、Ａｌ−Ｓｉ−Ｃｕ合金（ＡＣ４Ｂ、ＡＤＣ１０、ＡＤＣ１２）、Ａｌ−Ｓｉ−Ｍｇ合金（ＡＣ４Ｃ、ＡＣ４ＣＨ、ＡＤＣ３）Ａｌ−Ｓｉ−Ｃｕ−Ｍｇ−Ｎｉ合金（ＡＣ８Ａ、ＡＣ８Ｂ、ＡＣ８Ｃ、ＡＣ９Ａ、ＡＣ９Ｂ、ＡＤＣ１４）、Ａｌ−Ｍｇ合金（ＡＣ７Ａ、ＡＤＣ５、ＡＤＣ６）などを挙げることができる。   As aluminum or aluminum alloy, pure Al (1000 series), Al—Cu, Al—Cu—Mg series alloy (2000 series), Al—Mn, Al—Mn—Mg series alloy (3000 series) as specified by JIS ), Al-Si-Cu-Mg-Ni, Al-Si alloys (4000 series), Al-Mg alloys (5000 series), Al-Mg-Si alloys (6000 series), Al-Zn-Mg- Cu, Al-Zn-Mg alloy (7000 series), Al-Cu alloy (AC1A), Al-Cu-Mg alloy (AC1B), Al-Cu-Mg-Ni alloy (AC5A), Al-Si alloy (AC3A) , ADC1), Al-Cu-Si alloys (AC2A, AC2B), Al-Si-Cu alloys (AC4B, ADC10, ADC12), Al-Si-Mg alloys (AC4C, AC4CH) ADC3) Al-Si-Cu-Mg-Ni alloy (AC8A, AC8B, AC8C, AC9A, AC9B, ADC14), Al-Mg alloy (AC7A, ADC5, ADC6) and the like.

マグネシウムまたはマグネシウム合金としては、ＪＩＳで規格されている１〜７種を挙げることができる。
チタンまたはチタン合金としては、ＪＩＳで規格されている１〜４種を挙げることができる。Examples of magnesium or magnesium alloy include 1 to 7 types specified by JIS.
As titanium or a titanium alloy, 1-4 types specified by JIS can be mentioned.

二つの部材２、３は、前記した材料の中でも、ギア用途に用いられる鋼種で形成されるのが好ましい。なお、二つの部材２、３は、同じ鋼種で形成することもでき、異なる鋼種で形成することもできる。
二つの部材２、３は、ＤＬＣ膜５の形成を阻害するものでなければ、焼入れ、焼もどし、焼なまし、焼ならしなどの熱処理や、浸炭や窒化処理などを目的とした表面処理、さらには、研磨、ショットピーニング、エッチングなどの一般的な表面仕上処理を施すことができる。The two members 2 and 3 are preferably formed of a steel type used for gears among the materials described above. In addition, the two members 2 and 3 can also be formed with the same steel type, and can also be formed with different steel types.
If the two members 2 and 3 do not obstruct the formation of the DLC film 5, heat treatment such as quenching, tempering, annealing, normalizing, surface treatment for the purpose of carburizing or nitriding, Furthermore, general surface finishing treatments such as polishing, shot peening, and etching can be performed.

また、本発明の摺動部材１は、互いに摺動する二つ以上の部材２、３で構成されていればよく、これを構成する部材の数は制限されない。図１では、ステアリング装置のラックアンドピニオン摺動機構について二つの部材２、３を例示して説明しているが、例えば、図示しないリサーキュレーティングボール方式のステアリング装置のように、数多くの部材で構成されたものであっても、そのうちの一部の部材２の摺動面２ａにＤＬＣ膜５を形成すれば本発明の効果を奏することができる。なお、リサーキュレーティングボール方式のステアリング装置は、軸回りに回転し、その外周面に断面が半円形状を成す溝が螺旋状に形成されたボールシャフトと、円筒形状を成し、内側に前記したボールシャフトが挿入され、内周面に半円形状を成す溝が螺旋状に設けられたナットと、前記したボールシャフトの溝とナットの溝で形成される円形状の溝に入れられる数個から数十個のボールと、を含んで構成される。   Moreover, the sliding member 1 of this invention should just be comprised by the 2 or more members 2 and 3 which slide mutually, The number of the members which comprise this is not restrict | limited. In FIG. 1, the rack and pinion sliding mechanism of the steering device is described by exemplifying two members 2 and 3, but for example, there are many members such as a recirculating ball type steering device (not shown). Even if it is constituted, the effect of the present invention can be obtained if the DLC film 5 is formed on the sliding surface 2a of a part of the members 2 among them. The recirculating ball type steering device rotates around an axis, and has a ball shaft in which a groove having a semicircular cross-section is formed on the outer peripheral surface of the steering device, and a cylindrical shape. The nut is inserted into the inner peripheral surface and a semicircular groove is spirally provided on the inner peripheral surface, and several pieces can be inserted into the circular groove formed by the ball shaft groove and the nut groove. To dozens of balls.

摺動部材１の他の例示としては、図示はしないが、自動車用ステアリング機構として用いられる、ラックをスライドさせながら支持するラックガイドや、パワーアシスト機構駆動のためのウォームギア、ボールベアリング（転がり軸受け）などが挙げられる。また、スパーギアやベベルギアなどのギア機構や、接触面が移動する機構の摺動面などを挙げることができる。さらには、内燃機関のエンジンピストンリングの上下面およびピストンリング溝の少なくとも一方にＤＬＣ膜５を形成し、これらの間にグリース４を介在させることや、ピストンリング上下面およびピストン摩擦面の少なくとも一方にＤＬＣ膜５を形成し、これらの間にグリース４を介在させること、ピストンおよびピストンピン摩擦面の少なくとも一方にＤＬＣ膜５を形成し、これらの間にグリース４を介在させることなどが挙げられる。   Other examples of the sliding member 1 are not shown, but are used as a steering mechanism for an automobile, a rack guide that supports a rack while sliding it, a worm gear for driving a power assist mechanism, a ball bearing (rolling bearing). Etc. In addition, a gear mechanism such as a spur gear or a bevel gear, or a sliding surface of a mechanism in which a contact surface moves can be used. Furthermore, the DLC film 5 is formed on at least one of the upper and lower surfaces of the engine piston ring and the piston ring groove of the internal combustion engine, and the grease 4 is interposed therebetween, or at least one of the upper and lower surfaces of the piston ring and the piston friction surface. Forming a DLC film 5 between them and interposing the grease 4 between them, forming a DLC film 5 on at least one of the piston and piston pin friction surfaces, and interposing the grease 4 therebetween. .

一般的に、グリースとは、潤滑基油に増ちょう剤を拡散させて、常温で半固体または半流動性を有するゼリー状の潤滑剤とし、潤滑油より高い粘度を有するものをいう。   In general, grease refers to a jelly-like lubricant having a semi-solid or semi-fluid property at room temperature by diffusing a thickener in a lubricating base oil and having a higher viscosity than the lubricating oil.

ここで、潤滑基油は、鉱油系および合成油系のうちの少なくとも一方を用いることができる。鉱油系潤滑基油としては、ナフテン系鉱油、パラフィン系鉱油などが挙げられる。合成油系潤滑基油としては、合成炭化水素油、エステル油、エーテル油、ポリグリコール油、シリコーン油、フッ素油、パーフルオロポリエーテル油、ポリオレフィン油、ポリオールエステル油、植物油、流動パラフィンなどが挙げられる。潤滑基油は、一般的には７５〜９６質量％含有されている。   Here, as the lubricating base oil, at least one of a mineral oil system and a synthetic oil system can be used. Examples of the mineral oil base oil include naphthenic mineral oil and paraffinic mineral oil. Synthetic oil base lubricants include synthetic hydrocarbon oils, ester oils, ether oils, polyglycol oils, silicone oils, fluorine oils, perfluoropolyether oils, polyolefin oils, polyol ester oils, vegetable oils, liquid paraffins, etc. It is done. The lubricating base oil is generally contained in an amount of 75 to 96% by mass.

増ちょう剤は、セッケン系および非セッケン系のうちの少なくとも一方を用いることができる。
セッケン系増ちょう剤は、油脂または脂肪酸をアルカリ金属またはアルカリ土類金属の水酸化物でケン化したものである。これらの金属としては、ナトリウム、リチウム、カリウム、マグネシウム、カルシウムなどが挙げられるが、アルミニウムであってもよい。油脂または脂肪酸としては、ステアリン酸、１２−ヒドロキシステアリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、オレイン酸のうちの少なくとも一つが挙げられる。セッケン系増ちょう剤として具体的には、カルシウムセッケン、カルシウム複合セッケン、ナトリウムセッケン、アルミニウムセッケン、アルミニウム複合セッケン、リチウムセッケン、リチウム複合セッケンなどがある。
非セッケン系増ちょう剤は、有機系および無機系のうちの少なくとも一方を用いることができる。有機系の非セッケン系増ちょう剤としては、ウレア化合物（ポリウレア）、ナトリウムテレフタラメート、ＰＴＦＥ、インダスレン、フタロシアニンなどが挙げられる。無機系の非セッケン系増ちょう剤としては、有機物で表面処理されたベントナイト、シリカゲルなどが挙げられる。
なお、市販されているグリース中には増ちょう剤が約５〜２０質量％含有されている。本発明では、かかる含有量で増ちょう剤が含有されていれば所望の効果を得ることができるが、適宜含有量を増減させてもよい。As the thickener, at least one of soap and non-soap can be used.
The soap thickener is a saponified oil or fatty acid with an alkali metal or alkaline earth metal hydroxide. These metals include sodium, lithium, potassium, magnesium, calcium and the like, but may be aluminum. Examples of the oil or fatty acid include at least one of stearic acid, 12-hydroxystearic acid, lauric acid, myristic acid, palmitic acid, and oleic acid. Specific examples of the soap thickener include calcium soap, calcium composite soap, sodium soap, aluminum soap, aluminum composite soap, lithium soap and lithium composite soap.
As the non-soap thickener, at least one of an organic type and an inorganic type can be used. Examples of organic non-soap thickeners include urea compounds (polyurea), sodium terephthalamate, PTFE, indanthrene, phthalocyanine and the like. Examples of the inorganic non-soap thickener include bentonite and silica gel surface-treated with an organic substance.
The commercially available grease contains about 5 to 20% by mass of a thickener. In the present invention, a desired effect can be obtained as long as the thickener is contained in such a content, but the content may be increased or decreased as appropriate.

そして、本発明で用いるグリース４は、潤滑添加剤としてジアルキルジチオカルバミン酸モリブデン（Ｍｏ−ＤＴＣ）、ジチオリン酸モリブデン（Ｍｏ−ＤＴＰ）、二硫化モリブデン（ＭｏＳ2）、ポリテトラフルオロエチレン（ＰＴＦＥ）のうちの少なくとも一つを含有している。これらの潤滑添加剤はいずれも摩擦によるＤＬＣ膜５の結合構造の変化や摩擦化学反応によって層状構造物質になり得る成分または層状構造物質である。これらは、摺動時に摩擦界面や部材２、３の表面に生成されるトライボフィルムまたはその一部として機能することによって低摩擦化を具現する。また、耐摩耗性を向上させ、極圧性を向上させ、耐酸化性を向上させる機能も有する。これらの潤滑添加剤は、市販されているグリースに含まれ得るものであるが、任意に添加することもできる。The grease 4 used in the present invention includes, as lubricant additives, molybdenum dialkyldithiocarbamate (Mo-DTC), molybdenum dithiophosphate (Mo-DTP), molybdenum disulfide (MoS 2 ), and polytetrafluoroethylene (PTFE). Contains at least one of the following. Any of these lubricant additives is a component or a layered structure material that can be converted into a layered structure material by a change in the bonding structure of the DLC film 5 due to friction or a tribochemical reaction. These realize low friction by functioning as a tribo film generated on the friction interface or the surfaces of the members 2 and 3 or a part thereof when sliding. It also has the functions of improving wear resistance, extreme pressure, and oxidation resistance. These lubricating additives can be included in commercially available greases, but can be optionally added.

また、グリース４は、本発明の所望する効果を阻害しない範囲で前記した以外の添加剤として、極圧剤、酸化防止剤、防錆剤、金属不活性剤、粘着剤、構造改良剤などを含有させることもできる。なお、極圧剤としては、リン酸エステル、ジアルキルジチオリン酸、硫黄化合物塩化物などを挙げることができ、２〜１０質量％含有させることができる。油性剤としては、脂肪酸、エステルなどを挙げることができ、０．１〜５質量％含有させることができる。酸化防止剤としては、アミン化合物、フェノール、硫黄化合物、カルバメートなどを挙げることができ、０．１〜５質量％含有させることができる。防錆剤としては、スルホネート、アミン化合物、エステル類、脂肪酸などを挙げることができ、０．１〜５質量％含有させることができる。金属不活性剤としては、ベンゾトリアゾール、メルカプトチアゾールなどを挙げることができ、０．０５〜１質量％含有させることができる。粘着剤としては、ポリブテン、ポリイソブチレン、レジンなどを挙げることができ、０．５〜２質量％含有させることができる。構造改良剤としては、脂肪酸、グリセロール、グリコールなどを挙げることができ、０．１〜１．０質量％含有させることができる。   In addition, the grease 4 includes an extreme pressure agent, an antioxidant, a rust inhibitor, a metal deactivator, a pressure-sensitive adhesive, a structure improver, and the like as additives other than those described above as long as the desired effects of the present invention are not impaired. It can also be contained. In addition, as an extreme pressure agent, phosphate ester, dialkyl dithiophosphoric acid, sulfur compound chloride, etc. can be mentioned, and 2-10 mass% can be contained. Examples of the oily agent include fatty acids and esters, and can be contained in an amount of 0.1 to 5% by mass. Examples of the antioxidant include amine compounds, phenols, sulfur compounds, carbamates, and the like, and can be contained in an amount of 0.1 to 5% by mass. Examples of the rust inhibitor include sulfonates, amine compounds, esters, fatty acids and the like, and can be contained in an amount of 0.1 to 5% by mass. Examples of the metal deactivator include benzotriazole, mercaptothiazole and the like, and can be contained in an amount of 0.05 to 1% by mass. Examples of the pressure-sensitive adhesive include polybutene, polyisobutylene, and resin, and can be contained in an amount of 0.5 to 2% by mass. Examples of the structure improving agent include fatty acids, glycerol, glycols, and the like.

以上、本発明に係る摺動部材の一実施形態について説明した。一実施形態に係る摺動部材１によれば、低摩擦性に優れる。そのため、これを自動車等の摺動部分に適用すれば、滑らかなトルク伝達や静粛性などを得ることができ、自動車等の商品性を高めることができる。また、性質の異なるＤＬＣ膜５を複数層形成する必要がなく、グリースに含有される潤滑添加剤も特殊なものに限定されないため、安価且つ簡便に低摩擦性に優れた摺動部材１を提供することができる。
さらに、プラズマＣＶＤ法によってＤＬＣ膜５を成膜できるため、安価且つ簡便に、低摩擦性に優れた摺動部材１を製造することができる。Heretofore, an embodiment of the sliding member according to the present invention has been described. According to the sliding member 1 which concerns on one Embodiment, it is excellent in low-friction property. Therefore, if this is applied to a sliding portion of an automobile or the like, smooth torque transmission, quietness, etc. can be obtained, and the merchantability of the automobile or the like can be improved. Further, since it is not necessary to form a plurality of layers of DLC films 5 having different properties, and the lubricating additive contained in the grease is not limited to a special one, a sliding member 1 having excellent low friction properties can be provided at low cost. can do.
Furthermore, since the DLC film 5 can be formed by the plasma CVD method, the sliding member 1 excellent in low friction can be manufactured inexpensively and easily.

次に、本発明に係る摺動部材の効果を確認した実施例について具体的に説明する。
まず、ＳＵＪ２材からなる直径φ２０ｍｍのディスク材Ｄ（図２参照）の表面を鏡面研磨した。そして、鏡面研磨した表面の上に、表１に示す条件でＤＬＣ膜を成膜し、実施例１〜４および比較例１、２、４〜６に係るディスク材Ｄを作製した。なお、比較例３に係るディスク材ＤにはＤＬＣ膜を成膜しなかった。表１中のＣ2Ｈ2はアセチレン、Ｃ7Ｈ8はトルエン、ＣＨ4はメタンを表す。固体炭素としては等方性黒鉛を用いた。Next, an example in which the effect of the sliding member according to the present invention has been confirmed will be specifically described.
First, the surface of a disk material D (see FIG. 2) made of SUJ2 and having a diameter of 20 mm was mirror-polished. Then, a DLC film was formed on the mirror-polished surface under the conditions shown in Table 1, and disk materials D according to Examples 1 to 4 and Comparative Examples 1, 2, 4 to 6 were produced. Note that no DLC film was formed on the disk material D according to Comparative Example 3. In Table 1, C 2 H 2 represents acetylene, C 7 H 8 represents toluene, and CH 4 represents methane. Isotropic graphite was used as the solid carbon.

Figure 0006063376
Figure 0006063376

表１に示す潤滑添加剤を含有したグリースを実施例１〜４および比較例１〜６に係るディスク材ＤのＤＬＣ膜上に塗布し、ＳＵＪ２材からなる直径φ６ｍｍのボール材Ｂを用いて、図２に示すボールオンディスク摩擦摩耗試験を行った。なお、グリースの基剤は、合成炭化水素（ポリ−αオレフィン）にＬｉ系セッケンの増ちょう剤が添加されたものを用いた。ここで、表１に示されるＰＴＦＥとは、ポリテトラフルオロエチレンを表し、Ｍｏ系とは、ジアルキルジチオカルバミン酸モリブデン（Ｍｏ−ＤＴＣ）を表す。ＰＴＦＥは５質量％含有し、Ｍｏ系は５質量％含有していた。   Grease containing the lubricant additive shown in Table 1 was applied on the DLC film of the disk material D according to Examples 1 to 4 and Comparative Examples 1 to 6, and a ball material B having a diameter of 6 mm made of SUJ2 material was used. The ball-on-disk friction and wear test shown in FIG. 2 was performed. The grease base used was a synthetic hydrocarbon (poly-α olefin) with a Li-based soap thickener added. Here, PTFE shown in Table 1 represents polytetrafluoroethylene, and Mo-based represents molybdenum dialkyldithiocarbamate (Mo-DTC). PTFE contained 5% by mass, and Mo-based contained 5% by mass.

図２に示すボールオンディスク摩擦摩耗試験は、ボール材Ｂへの荷重を５Ｎとし、ディスク材Ｄの摺動速度を１００ｍｍ／秒とし、温度条件を２５℃として１００００サイクル（５０ｍｉｎ）行った。実施例１〜４および比較例１〜６についてボールオンディスク摩擦摩耗試験を３回行い、摩擦係数の平均値を求めた。摩擦係数の平均値は、ディスク材Ｄ上にＤＬＣ膜を形成していない比較例３を基準とし、０．１１０以下を合格、０．１１０を超えるものを不合格とした。   The ball-on-disk frictional wear test shown in FIG. 2 was performed for 10000 cycles (50 min) with a load on the ball material B of 5 N, a sliding speed of the disk material D of 100 mm / second, and a temperature condition of 25 ° C. About Examples 1-4 and Comparative Examples 1-6, the ball-on-disk frictional wear test was done 3 times, and the average value of the friction coefficient was calculated | required. The average value of the friction coefficient was based on Comparative Example 3 in which the DLC film was not formed on the disk material D, and 0.110 or less was accepted and those exceeding 0.110 were rejected.

また、実施例１〜４および比較例１〜６のＤＬＣ膜のヤング率は、ＩＳＯ １４５７７に準拠したナノインデンターを用いて測定した。
実施例１〜４および比較例１〜６のＤＬＣ膜の水素含有量は、ラザフォード後方散乱分光法（Rutherford Backscattering Spectrometry；ＲＢＳ）により測定した。ＲＢＳでは、試料にヘリウム（Ｈe）イオンを照射して、特に水素含有量については、反跳して前方に散乱した水素を検出した結果より算出した。Moreover, the Young's modulus of the DLC film of Examples 1-4 and Comparative Examples 1-6 was measured using the nano indenter based on ISO14577.
The hydrogen contents of the DLC films of Examples 1 to 4 and Comparative Examples 1 to 6 were measured by Rutherford Backscattering Spectrometry (RBS). In RBS, the sample was irradiated with helium (He) ions, and particularly the hydrogen content was calculated from the results of detecting hydrogen recoiled and scattered forward.

実施例１〜４および比較例１〜６のＤＬＣ膜の成膜条件（製法、原料ガス、ガス圧力［Ｐａ］、バイアス電圧、プラズマ出力［Ｗ］またはアーク電圧［Ｖ］）、水素含有量［ａｔ％］、ヤング率［ＧＰａ］、グリースに含有された潤滑添加剤の種類および摩擦係数（平均値）を前記表１に併せて示した。   Film formation conditions (production method, source gas, gas pressure [Pa], bias voltage, plasma output [W] or arc voltage [V]), hydrogen content [Examples 1 to 4 and Comparative Examples 1 to 6] at%], Young's modulus [GPa], types of lubricant additives contained in the grease, and friction coefficient (average value) are also shown in Table 1 above.

表１に示すように、実施例１〜４は、いずれも本発明の要件を満たしているので、摩擦係数が小さかった。
これに対して、比較例１、２は、ヤング率が２００ＧＰａ未満であったため、摩擦係数が大きくなった。これは、ＤＬＣ膜の硬さが低かったため、ＤＬＣ膜の炭素成分の黒鉛質物質への構造変化が不十分であり、同時に、潤滑添加剤の摩擦化学反応が十分に進行しなかったことによると考えられる。
また、比較例３は、ディスク材の表面にＤＬＣ膜を形成しなかったため、摩擦係数が大きくなった。
そして、比較例４は、グリースが本発明で狙いとするような潤滑添加剤を含有していないため、摩擦係数が大きくなった。
なお、比較例５、６は、いずれも摩擦係数は合格していたものの、ＤＬＣ膜のヤング率が高過ぎるため、相手攻撃性が大きく、長期使用により相手材の摩耗が激しくなることが予想されるので好ましくないと判断された。As shown in Table 1, since Examples 1 to 4 all satisfied the requirements of the present invention, the friction coefficient was small.
On the other hand, Comparative Examples 1 and 2 had a higher coefficient of friction because the Young's modulus was less than 200 GPa. This is because the structural change of the carbon component of the DLC film to the graphite material was insufficient because the hardness of the DLC film was low, and at the same time, the tribochemical reaction of the lubricant additive did not proceed sufficiently. Conceivable.
In Comparative Example 3, since the DLC film was not formed on the surface of the disk material, the friction coefficient was increased.
And since the comparative example 4 did not contain the lubricating additive which grease aims at by this invention, the friction coefficient became large.
Although Comparative Examples 5 and 6 both passed the friction coefficient, the DLC film has a too high Young's modulus, so the opponent's aggression is large, and the wear of the counterpart material is expected to become severe after long-term use. Therefore, it was judged unfavorable.

表１の実施例１〜４および比較例１〜４について、ヤング率と摩擦係数の関係を示したのが、図３のグラフである。なお、ＤＬＣ膜を形成していない比較例３は、ＤＬＣ膜のヤング率でもってプロットすることができないので、その摩擦係数０．１１０を同図中に破線で示した。また、ＤＬＣ膜のヤング率が極端に大きい比較例５、６は図示していない。同図中、◆および◇のプロットは、潤滑添加剤としてＰＴＦＥを添加していることを表し、■のプロットは、潤滑添加剤としてＭｏ系を添加していることを表し、○のプロットは、潤滑添加剤を添加していないことを表している。   The graph of FIG. 3 shows the relationship between the Young's modulus and the friction coefficient for Examples 1 to 4 and Comparative Examples 1 to 4 in Table 1. In Comparative Example 3 in which the DLC film was not formed, it was not possible to plot with the Young's modulus of the DLC film, so the friction coefficient 0.110 was indicated by a broken line in FIG. Further, Comparative Examples 5 and 6 in which the Young's modulus of the DLC film is extremely large are not shown. In the figure, ◆ and ◇ plots indicate that PTFE is added as a lubricant additive, ■ plots indicate that a Mo-based additive is added as a lubricant additive, and ○ plots are This means that no lubricant additive is added.

図３および表１に示すように、本発明の要件を満たす実施例１〜４は、ＤＬＣ膜のヤング率が大きくなるにつれて摩擦係数が小さくなり、同図中で示すように右肩下がりの分布となっている。これに対し、ヤング率が２００ＧＰａ未満の比較例１、２は、潤滑添加剤が添加されたグリースを用いていても、摩擦係数が十分小さくならなかった。   As shown in FIG. 3 and Table 1, in Examples 1 to 4 that satisfy the requirements of the present invention, the coefficient of friction decreases as the Young's modulus of the DLC film increases, and as shown in FIG. It has become. On the other hand, Comparative Examples 1 and 2 having Young's modulus of less than 200 GPa did not have a sufficiently small friction coefficient even when using a grease to which a lubricating additive was added.

そして、表１の実施例１〜４および比較例１〜６について、ＤＬＣ膜の水素含有量と摩擦係数の関係を示したのが、図４のグラフである。なお、ＤＬＣ膜を形成していない比較例３は、ＤＬＣ膜のヤング率でもってプロットすることができないので、その摩擦係数０．１１０を同図中に破線で示した。同図中、◆および◇のプロットは、潤滑添加剤としてＰＴＦＥを添加していることを表し、■および□のプロットは、潤滑添加剤としてＭｏ系を添加していることを表し、○のプロットは、潤滑添加剤を添加していないことを表している。   The graph of FIG. 4 shows the relationship between the hydrogen content of the DLC film and the friction coefficient for Examples 1 to 4 and Comparative Examples 1 to 6 in Table 1. In Comparative Example 3 in which the DLC film was not formed, it was not possible to plot with the Young's modulus of the DLC film, so the friction coefficient 0.110 was indicated by a broken line in FIG. In the figure, ◆ and ◇ plots indicate that PTFE is added as a lubricant additive, ■ and □ plots indicate that a Mo-based additive is added as a lubricant additive, and ○ plots Indicates that no lubricant additive is added.

図４および表１に示すように、本発明の要件を満たす実施例１〜４は、ＤＬＣ膜の水素含有量が小さいほど摩擦係数も小さくなる。しかしながら、ＤＬＣ膜の水素含有量が１５ａｔ％未満になると、同図中の比較例５、６のように期待されるほど摩擦係数が小さくならなかった。これは、ＤＬＣ膜が過度に硬いため相手攻撃性が大きく、相手材の摩耗量が増大したためと考えられる。   As shown in FIG. 4 and Table 1, in Examples 1 to 4 that satisfy the requirements of the present invention, the smaller the hydrogen content of the DLC film, the smaller the friction coefficient. However, when the hydrogen content of the DLC film was less than 15 at%, the friction coefficient did not decrease as expected as in Comparative Examples 5 and 6 in the figure. This is presumably because the DLC film is excessively hard, so that the opponent's aggressiveness is large and the wear amount of the counterpart material is increased.

次に、ＤＬＣ膜を形成したピニオンギア部品（実施例５）とラック部品を組み合わせ、ラックアンドピニオン摺動機構におけるピニオンシャフトのフリクショントルクを測定した。なお、ピニオンギア部品へのＤＬＣ膜の形成は、実施例１と同じ条件で行い、グリースには、潤滑添加剤として少なくとも有機モリブデンおよび二硫化モリブデンの混合物と、ＰＴＦＥとが添加されている協同油脂社製マルテンプＡＣ−Ｐを使用した。ＤＬＣ膜を形成していないピニオンギア部品（比較例７）を用いた場合のフリクショントルクも同様に測定した。実施例５と比較例７のフリクショントルク［Ｎ・ｍ］を図５に示す。なお、同図中、横軸はピニオンギア部品の回転角度［°］を表し、縦軸はフリクショントルク［Ｎ・ｍ］を表している。   Next, the pinion gear part (Example 5) on which the DLC film was formed and the rack part were combined, and the friction torque of the pinion shaft in the rack and pinion sliding mechanism was measured. The DLC film is formed on the pinion gear parts under the same conditions as in Example 1, and the grease is a Kyodo Yushi in which at least a mixture of organic molybdenum and molybdenum disulfide and PTFE are added as lubricant additives. Martemp AC-P made by the company was used. The friction torque when using a pinion gear part (Comparative Example 7) in which no DLC film was formed was also measured in the same manner. The friction torque [N · m] of Example 5 and Comparative Example 7 is shown in FIG. In the figure, the horizontal axis represents the rotation angle [°] of the pinion gear part, and the vertical axis represents the friction torque [N · m].

比較例７のフリクショントルクは約１．６Ｎ・ｍであった。また、比較例７のフリクショントルクは周期的に変動し、終始安定していなかった。
これに対し、実施例５のフリクショントルクは、比較例７の約２０％減となる約１．２〜１．３Ｎ・ｍであった。また、フリクショントルクの変動が殆どなく、終始安定していた。The friction torque of Comparative Example 7 was about 1.6 N · m. Further, the friction torque of Comparative Example 7 periodically fluctuated and was not stable throughout.
On the other hand, the friction torque of Example 5 was about 1.2 to 1.3 N · m, which is about 20% lower than that of Comparative Example 7. Further, there was almost no fluctuation of the friction torque, and it was stable from the beginning.

以上に説明したように、本発明の要件を満たす実施例は、低摩擦性に優れることがわかった。そのため、これを自動車等の摺動部分に適用すれば、滑らかなトルク伝達や静粛性などを得ることができ、自動車等の商品性を高めることが示唆された。また、性質の異なるＤＬＣ膜を複数層形成する必要がなく、グリースに含有される潤滑添加剤も特殊なものに限定されないため、安価且つ簡便に低摩擦性に優れた摺動部材を提供できることが示唆された。
さらに、プラズマＣＶＤ法によってＤＬＣ膜を成膜でき、安価且つ簡便に、低摩擦性に優れた摺動部材を製造できることが示唆された。As described above, it was found that the examples satisfying the requirements of the present invention are excellent in low friction. Therefore, it has been suggested that if this is applied to a sliding portion of an automobile or the like, smooth torque transmission, quietness, etc. can be obtained, and the merchantability of the automobile or the like is improved. Further, it is not necessary to form a plurality of DLC films having different properties, and the lubricating additive contained in the grease is not limited to a special one, so that it is possible to provide a sliding member excellent in low friction property at low cost. It was suggested.
Furthermore, it was suggested that a DLC film can be formed by a plasma CVD method, and that a sliding member excellent in low friction can be manufactured inexpensively and easily.

１ 摺動部材
２ 部材
２ａ 摺動面
３ 部材
４ グリース
５ ＤＬＣ膜（非晶質硬質炭素膜）DESCRIPTION OF SYMBOLS 1 Sliding member 2 Member 2a Sliding surface 3 Member 4 Grease 5 DLC film (amorphous hard carbon film)

Claims (2)

相対する二つの部材の間にジアルキルジチオカルバミン酸モリブデン、ジチオリン酸モリブデン、二硫化モリブデン、ポリテトラフルオロエチレンのうちの少なくとも一つを潤滑添加剤として含有し、銅系の添加剤を含有しないグリースを介在させて互いに摺動する摺動部材であって、
前記二つの部材のうちの少なくとも一つの部材の摺動面に、水素を１７〜２９原子％含み、ヤング率が２０１ＧＰａ以上２５３ＧＰａ以下、膜厚が０．５〜２０μｍである非晶質硬質炭素膜を形成したことを特徴とする摺動部材。 A grease containing at least one of molybdenum dialkyldithiocarbamate, molybdenum dithiophosphate, molybdenum disulfide, and polytetrafluoroethylene as a lubricating additive and no copper-based additive is interposed between two opposing members. Sliding members that slide relative to each other,
An amorphous hard carbon film containing 17 to 29 atomic% of hydrogen, Young's modulus of 201 GPa to 253 GPa , and a film thickness of 0.5 to 20 μm on the sliding surface of at least one of the two members The sliding member characterized by forming. 相対する二つの部材の間にジアルキルジチオカルバミン酸モリブデン、ジチオリン酸モリブデン、二硫化モリブデン、ポリテトラフルオロエチレンのうちの少なくとも一つを潤滑添加剤として含有し、銅系の添加剤を含有しないグリースを介在させて互いに摺動する摺動部材であって、
前記二つの部材のうちの少なくとも一つの部材の摺動面に、水素を含み、ヤング率が２０１ＧＰａ以上２５３ＧＰａ以下、前記グリースを介在させた摩擦係数が０．０５７以上０．１０６以下、膜厚が０．５〜２０μｍである非晶質硬質炭素膜を形成したことを特徴とする摺動部材。 A grease containing at least one of molybdenum dialkyldithiocarbamate, molybdenum dithiophosphate, molybdenum disulfide, and polytetrafluoroethylene as a lubricating additive and no copper-based additive is interposed between two opposing members. Sliding members that slide relative to each other,
The sliding surface of at least one of the two members contains hydrogen, the Young's modulus is 201 GPa or more and 253 GPa or less, the friction coefficient with the grease interposed is 0.057 or more and 0.106 or less , and the film thickness is A sliding member comprising an amorphous hard carbon film having a thickness of 0.5 to 20 μm .
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